US1092791A - Extraction of glycerin and fatty matters contained in distillery-vinasses. - Google Patents
Extraction of glycerin and fatty matters contained in distillery-vinasses. Download PDFInfo
- Publication number
- US1092791A US1092791A US6?020?11A US1092791DA US1092791A US 1092791 A US1092791 A US 1092791A US 1092791D A US1092791D A US 1092791DA US 1092791 A US1092791 A US 1092791A
- Authority
- US
- United States
- Prior art keywords
- glycerin
- vinasses
- extraction
- distillery
- fatty matters
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 title description 29
- 235000011187 glycerol Nutrition 0.000 title description 15
- 238000000605 extraction Methods 0.000 title description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- 229960005150 glycerol Drugs 0.000 description 14
- 235000019441 ethanol Nutrition 0.000 description 11
- 239000002904 solvent Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000003925 fat Substances 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 4
- 238000004821 distillation Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 150000007524 organic acids Chemical class 0.000 description 3
- 235000005985 organic acids Nutrition 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- 229910001864 baryta Inorganic materials 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 235000013379 molasses Nutrition 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241000283690 Bos taurus Species 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- GXCLVBGFBYZDAG-UHFFFAOYSA-N N-[2-(1H-indol-3-yl)ethyl]-N-methylprop-2-en-1-amine Chemical compound CN(CCC1=CNC2=C1C=CC=C2)CC=C GXCLVBGFBYZDAG-UHFFFAOYSA-N 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- -1 ferric. hydrate Substances 0.000 description 1
- 150000002314 glycerols Chemical class 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 235000011182 sodium carbonates Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical compound [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
Definitions
- GASTON PHILIPPE GUIGNARD a citizen of the Republic of France, and a resident of Avenuedes Marronniers, Melun, Seine-et-Marne, France,
- the invention has for object the simultaneous extraction of the glycerin and the fatty matters and in some cases of the betain contained in distillery vinasses, and consists in submitting them to a total desiccation followed by lye-washin by means of a mixture of anhydrous et yl alcohol with addition of acetone, and carbon tetrachlorid or other solvent of fatty matters soluble'in alcohol.
- a suitable re-agent such as ferric. hydrate, lime, baryta, etc.
- Grain-vinasses are treated as follows: To the vinasses leaving the distilling column there is added zinc oxid, ferric hydrate,
- dry malt from which the fats and glycerin are extracted by washing preferably in an extractor, with anhydrous ethyl alcohol and acetone, or anhydrous ethyl alcohol and carbon tetrachlorid, or a mixture of the three solvents.
- the solvent liquid removes the fats and the glycerin; the insoluble portion consisting of nitrogenous matter, cellulose, etc, may be used for feedin cattle.
- the solvent is recovered by distillation leaving a syrupy liquid upon which the fats" float: the two parts are separated by decantation yielding fat and glycerin.
- the glycerin is purified in either of the following ways: (1) by distillation in 'cacuo at 179-180". (2) by passing this glycerin through the above mentioned drying apparatus heated below 100 and in 'vacuo; the residue leaving the apparatus is finally treated with the mixture of alcohol and carbon tetrachlorid. Pure glycerin is recovered by evaporation.
- the process for the treatment of molasses I and beet-vinasses is the same as that for grain-Vin es up to the treatment with the mixture of, said solvent liquids inclusive.
- the washing of these liquids in the extractor yields: (1) a solution containing glyc erin and betain. (2) an insoluble portion comprising sodium and potassiumcarbonates, etc., and various non-nitrogenous organic substances.
- the separation of the glycerin and betain is effected by evaporating the solvent; the residue when completely dried is treated again with carbon tetrachlorid alone which dissolves only the betain.
- the residue is glycerin which is purified as. above described.
- the part insoluble in the solvent is dissolved in the minimum quantity of water and saturated with carbon dioxid.
- the sodium and potassium salts yield insoluble bicarbon zitfis e mother liquors of this treatment serve for the solution of the part insoluble in alcohol in the following operation.
- a process for the simultaneous extraction of glycerin and fatty matters from vinasses comprising the separation of organic acids by precipitationwith a suitable.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Extraction Or Liquid Replacement (AREA)
Description
GA TON PHILIPPE GUIGNARD; or MELUN, Am) HENRI LOUIS ADOLPHE MARIE WATRIGANT, or LILLE', FRANCE.
EXTRACTION or GLYCERIN' AND FATTY MATTERS corrr'amnn m nIsTrLLnnY- i VI'NASSES.
Ere-eater.
No Drawing.
Specification of Letters Patent.
Patented Apr. 7, 119%.
To all whom it may concern Be it known that we, GASTON PHILIPPE GUIGNARD, a citizen of the Republic of France, and a resident of Avenuedes Marronniers, Melun, Seine-et-Marne, France,
and HENRI Lotus ADOLPI-IE MARIE VVATRI- oAnT, a citizen of the Republic of France, and a resident of i8 Facade de lEsplanade, Lille, Nord, France, have invented a new and useful Process for the Extraction of Glycerin and Fatty Matters Contained in Distillery-vinasses, of which the following is a specification.
The invention has for object the simultaneous extraction of the glycerin and the fatty matters and in some cases of the betain contained in distillery vinasses, and consists in submitting them to a total desiccation followed by lye-washin by means of a mixture of anhydrous et yl alcohol with addition of acetone, and carbon tetrachlorid or other solvent of fatty matters soluble'in alcohol.
ethyl alcohol and thereby to avoid solution by the solvent of bodies soluble in aqueous alcohol.
In practice it is advisable first to separate the organic acids (succinic, tartaric,
citric, etc.,) contained in the vinasses by,
precipitating them with a suitable re-agent such as ferric. hydrate, lime, baryta, etc.
These organic acids are separated from one another as hereafter described.
The following description indicates two examples of the application of the invention, one to grain-vinasses and the other to beetvinasses and molasses.
Grain-vinasses are treated as follows: To the vinasses leaving the distilling column there is added zinc oxid, ferric hydrate,
lime or baryta, and if desired a mixture of. these two bases; the excess is saturated with The total desiccation has for object to prevent hydration of the anhydrous -which are separated by filtration.
called dry malt, from which the fats and glycerin are extracted by washing preferably in an extractor, with anhydrous ethyl alcohol and acetone, or anhydrous ethyl alcohol and carbon tetrachlorid, or a mixture of the three solvents. The solvent liquid removes the fats and the glycerin; the insoluble portion consisting of nitrogenous matter, cellulose, etc, may be used for feedin cattle. The solvent is recovered by distillation leaving a syrupy liquid upon which the fats" float: the two parts are separated by decantation yielding fat and glycerin.
The glycerin is purified in either of the following ways: (1) by distillation in 'cacuo at 179-180". (2) by passing this glycerin through the above mentioned drying apparatus heated below 100 and in 'vacuo; the residue leaving the apparatus is finally treated with the mixture of alcohol and carbon tetrachlorid. Pure glycerin is recovered by evaporation.
The process for the treatment of molasses I and beet-vinasses is the same as that for grain-Vin es up to the treatment with the mixture of, said solvent liquids inclusive. The washing of these liquids in the extractor yields: (1) a solution containing glyc erin and betain. (2) an insoluble portion comprising sodium and potassiumcarbonates, etc., and various non-nitrogenous organic substances. The separation of the glycerin and betain is effected by evaporating the solvent; the residue when completely dried is treated again with carbon tetrachlorid alone which dissolves only the betain. The residue is glycerin which is purified as. above described. The part insoluble in the solvent is dissolved in the minimum quantity of water and saturated with carbon dioxid. The sodium and potassium salts yield insoluble bicarbon zitfis e mother liquors of this treatment serve for the solution of the part insoluble in alcohol in the following operation.
Having thus described our invention, what we claim as such d desire to secure by Letters Patent is i Y 1. The simultaneous extraction of glycerin and fatty matters contained in distilmeans of amixture of anhydrous ethyl alcohol and a solvent of the fatty matters soluole in alcohol.
2. A process for the simultaneous extraction of glycerin and fatty matters from vinasses, comprising the separation of organic acids by precipitationwith a suitable.
base, the filtration and evaporation to dryness of the vinasses, the extraction of the dried residue with anhydrous ethyl alcohol mixed with a solvent soluble therein, the removal by distillation of the mixed solvent,
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US1092791TA |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US1092791A true US1092791A (en) | 1914-04-07 |
Family
ID=3161003
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US6?020?11A Expired - Lifetime US1092791A (en) | Extraction of glycerin and fatty matters contained in distillery-vinasses. |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US1092791A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2436209A (en) * | 1943-09-18 | 1948-02-17 | Colgate Palmolive Peet Co | Extraction of polyhydric alcohols |
| US2478417A (en) * | 1938-02-24 | 1949-08-09 | Colgate Palmolive Peet Co | Process of recovering glycerine from fermentation concentrates |
| US2479041A (en) * | 1943-09-18 | 1949-08-16 | Colgate Palmolive Peet Co | Glycerine extraction process |
| FR2964657A1 (en) * | 2010-09-15 | 2012-03-16 | Rhodia Operations | PROCESS FOR PURIFYING RAW GLYCEROL |
-
0
- US US6?020?11A patent/US1092791A/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2478417A (en) * | 1938-02-24 | 1949-08-09 | Colgate Palmolive Peet Co | Process of recovering glycerine from fermentation concentrates |
| US2436209A (en) * | 1943-09-18 | 1948-02-17 | Colgate Palmolive Peet Co | Extraction of polyhydric alcohols |
| US2479041A (en) * | 1943-09-18 | 1949-08-16 | Colgate Palmolive Peet Co | Glycerine extraction process |
| FR2964657A1 (en) * | 2010-09-15 | 2012-03-16 | Rhodia Operations | PROCESS FOR PURIFYING RAW GLYCEROL |
| WO2012034904A1 (en) * | 2010-09-15 | 2012-03-22 | Rhodia Operations | Process for purifying crude glycerol |
| CN103097327A (en) * | 2010-09-15 | 2013-05-08 | 罗地亚经营管理公司 | Process for purifying crude glycerol |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US1092791A (en) | Extraction of glycerin and fatty matters contained in distillery-vinasses. | |
| US3422090A (en) | Process of producing esters from plants of the genus valeriana | |
| US2517276A (en) | Process for the purification of 1-ascorbic acid | |
| GB786547A (en) | Stabilizing levulinic acid during heating | |
| US1193951A (en) | Mantteacttnie os by-jpb | |
| GB774809A (en) | A continuous process for the production of furfural and acetic acid from pentosan-containing material | |
| US2223797A (en) | Recovery of lactic acids from crude solutions thereof | |
| DE1768412C3 (en) | Process for the production of vinyl acetate | |
| US1078580A (en) | Process of extracting glycerin from vinasses. | |
| US2806890A (en) | Recovering trimethylolethane by ethyl acetate extraction | |
| US1858151A (en) | Process for concentrating volatile aliphatic acids | |
| Robinson | Two Compounds Isolated from Peat Soils. | |
| US3337366A (en) | Recovering sugars from aqueous pulping liquor containing lignosulfonates using acetone | |
| US1147768A (en) | Process of obtaining by-products from distillery-slop. | |
| US2389173A (en) | Recovery of glycerol from fermented liquors | |
| US3266933A (en) | Process for the extraction of aqueous sugar solution resulting from the hydrolysis of lignocellulosic material | |
| US2114825A (en) | Process for partial dehydration of acetic acid and other lower fatty acids | |
| US345810A (en) | Franz schwengers | |
| US2156345A (en) | Concentration of aliphatic acids | |
| US2249525A (en) | Purification of vitamin a esters | |
| US2359126A (en) | Process of obtaining purified flavanone glucosides | |
| US3474142A (en) | Processes for preparation of acrylamide | |
| US1884561A (en) | Process for the recovery of ammonia from fermentation mashes | |
| US1147769A (en) | Manufacture of by-products from distillery-slop. | |
| DE552888C (en) | Process for the preparation of esters |